TY - JOUR
T1 - Living with breakthrough
T2 - Two-dimensional liquid-chromatography separations of a water-soluble synthetically grafted bio-polymer
AU - van de Ven, H. C.
AU - Purmova, J.
AU - Groeneveld, G.
AU - Bos, Tijmen S.
AU - Gargano, A. F.G.
AU - van der Wal, Sj
AU - Mengerink, Y.
AU - Schoenmakers, Peter J.
PY - 2020/9
Y1 - 2020/9
N2 - In this study, we evaluate the use of various two-dimensional liquid chromatographic methods to characterize water-soluble, synthetically grafted bio-polymers, consisting of long poly(acrylic acid) chains and short maltodextrin grafts. The confirmation of the presence of grafting and the estimation of its extent is challenging. It is complicated by the limited solubility of polymers, their structural dispersity and chemical heterogeneity. Moreover, the starting materials (and other reagents, reaction products and additives) may be present in the product. Reversed-phase liquid chromatography (RPLC), hydrophilic-interaction liquid chromatography (HILIC) and size-exclusion chromatography (SEC) were used to characterize the product, as well as the starting materials. Additionally, fractions were collected for off-line characterization by infrared spectroscopy and mass spectrometry. The one-dimensional separation methods were found to be inconclusive regarding the grafting question. Breakthrough (the early elution of polymer fractions due to strong injection solvents) is shown to be a perpetual problem. This issue is not solved by comprehensive two-dimensional liquid chromatography (LC × LC), but information demonstrating the success of the grafting reaction could be obtained. SEC × RPLC and HILIC × RPLC separations are presented and discussed.
AB - In this study, we evaluate the use of various two-dimensional liquid chromatographic methods to characterize water-soluble, synthetically grafted bio-polymers, consisting of long poly(acrylic acid) chains and short maltodextrin grafts. The confirmation of the presence of grafting and the estimation of its extent is challenging. It is complicated by the limited solubility of polymers, their structural dispersity and chemical heterogeneity. Moreover, the starting materials (and other reagents, reaction products and additives) may be present in the product. Reversed-phase liquid chromatography (RPLC), hydrophilic-interaction liquid chromatography (HILIC) and size-exclusion chromatography (SEC) were used to characterize the product, as well as the starting materials. Additionally, fractions were collected for off-line characterization by infrared spectroscopy and mass spectrometry. The one-dimensional separation methods were found to be inconclusive regarding the grafting question. Breakthrough (the early elution of polymer fractions due to strong injection solvents) is shown to be a perpetual problem. This issue is not solved by comprehensive two-dimensional liquid chromatography (LC × LC), but information demonstrating the success of the grafting reaction could be obtained. SEC × RPLC and HILIC × RPLC separations are presented and discussed.
KW - Breakthrough
KW - Grafted bio-polymer
KW - HILIC × RPLC
KW - LC × LC
KW - Polyacrylic acid–maltodextrin hybrid
KW - SEC × RPLC
UR - http://www.scopus.com/inward/record.url?scp=85090743213&partnerID=8YFLogxK
UR - http://www.scopus.com/inward/citedby.url?scp=85090743213&partnerID=8YFLogxK
U2 - 10.3390/separations7030041
DO - 10.3390/separations7030041
M3 - Article
AN - SCOPUS:85090743213
SN - 2297-8739
VL - 7
SP - 1
EP - 16
JO - Separations
JF - Separations
IS - 3
M1 - 41
ER -
